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A new boronate-affinity hollow solid phase extraction adsorbent for the enrichment of cis-diol-containing isoflavones in soybean milk samples

机译:一种用于富集豆浆样品中富含顺式二醇的异黄酮的新型硼酸酯亲和空心固相萃取吸附剂

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In this study, a new boronate-affinity hollow adsorbent was successfully fabricated. This adsorbent was prepared using mesoporous MCM-48 as a sacrificial support, methacrylic acid (MAA), N,N-methylenebisacrylamide (MBA) and azobisisobutyronitrile (AIBN) were applied as a functional monomer, cross-linker and initiator, respectively, and further modified with boronic acid groups (4-vinylphenylboronic acid, VPBA) to improve the enrichment efficiency. Such materials were composed of a hollow structure, a hydrophilic polymer coating of poly(MBA-MAA), and a VPBA-functionalized shell designed for capturing isoflavones. The resulting material coupled with high-performance liquid chromatography (HPLC) was applied to analyze three cis-diol isoflavones (daidzin, glycitin, and genistin) in soybean milk samples. The sorbent was characterized by transmission electron microscopy, Fourier transform infrared spectrometry and thermo-gravimetric analysis. Several parameters affecting the extraction efficiency were optimized. Owing to the hollow structure, more binding sites were located on the inner and outer surfaces of this material, which could facilitate the binding of the target molecules to the adsorbent. Adsorption selectivity studies indicated that the prepared material can selectively recognize isoflavones. Under optimized conditions, the limits of detection of the method were 3.8 to 7.3 μg L?1 for the three isoflavones based on a signal-to-noise ratio of 3?:?1. The spiked recoveries were found to be between 67.4 and 104.7% (the relative standard deviations were less than 3.8%, n = 3). This indicated the superiority of the method in selective extraction of isoflavones even from complex matrices.
机译:在这项研究中,成功​​地制造了一种新型的硼酸亲和空心吸附剂。该吸附剂是使用中孔MCM-48作为牺牲性载体制备的,分别使用甲基丙烯酸(MAA),N,N-亚甲基双丙烯酰胺(MBA)和偶氮二异丁腈(AIBN)作为功能单体,交联剂和引发剂,并进一步使用用硼酸基团(4-乙烯基苯基硼酸,VPBA)改性以提高富集效率。这类材料由空心结构,聚(MBA-MAA)的亲水性聚合物涂层和为捕获异黄酮而设计的VPBA官能化壳组成。将所得材料与高效液相色谱(HPLC)结合使用,以分析豆浆样品中的三种顺式-二醇异黄酮(大豆苷,甘草肽和染料木素)。通过透射电子显微镜,傅立叶变换红外光谱和热重分析对吸附剂进行了表征。优化了影响萃取效率的几个参数。由于中空结构,更多的结合位点位于该材料的内表面和外表面,这可以促进目标分子与吸附剂的结合。吸附选择性研究表明,所制备的物质可以选择性地识别异黄酮。在最佳条件下,基于3?:?1的信噪比,三种异黄酮的检测限为3.8至7.3μgL?1。发现加标回收率在67.4和104.7%之间(相对标准偏差小于3.8%,n = 3)。这表明该方法在从复杂基质中选择性提取异黄酮方面的优势。

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